CN109593975A - Using the method for steel slag and vanadine mixing vanadium extraction - Google Patents
Using the method for steel slag and vanadine mixing vanadium extraction Download PDFInfo
- Publication number
- CN109593975A CN109593975A CN201811529300.3A CN201811529300A CN109593975A CN 109593975 A CN109593975 A CN 109593975A CN 201811529300 A CN201811529300 A CN 201811529300A CN 109593975 A CN109593975 A CN 109593975A
- Authority
- CN
- China
- Prior art keywords
- vanadium
- steel slag
- vanadine
- slag
- thin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a kind of methods of steel slag and the vanadium extraction of vanadine mixture, comprising: pretreatment, mixing, roasting, leaching, precipitation, is dried deamination and melted broken, milling.Extraction process of the invention can efficiently use the vanadium iron resources in steel slag, be processed as valuable material, increased economic efficiency, and reduce energy consumption, reduce environmental pollution, can also promote the development of other relevant industries.Vanadium recovery rate of the present invention reaches 95% or more.The present invention comprehensively utilizes vanadine and steel slag, realizes recycling for vanadium resource, has high economic benefit and social benefit.
Description
Technical field
The present invention relates to a kind of methods of vanadium extraction, belong to metal smelt technology.Raw material is mainly steel slag and vanadine mixture.
Background technique
Vanadium is a kind of important valuable metal element, has the physics such as excellent tensile strength, hardness and yield strength
Mechanical property is a kind of important alloy added material.Steel slag is one of the source of industrial vanadium.The steel slag of different smelteries
Ingredient is different.In the steel slag for climbing steel supply, TFe about 32 ~ 40%, V2O5About 16 ~ 18%, SiO2About 15 ~ 17%, TiO2About
12.50%, CaO about 1.5 ~ 2.5%, MgO about 3 ~ 5%, MnO about 8 ~ 10%, Cr2O3About 1 ~ 1.5%.Converter slag is generally comprised containing vanadium point
Spar phase, silicate phase, metal iron phase and Free quartz phase.
In existing technical literature, " steel converter vanadium slag production V is climbed2O5Technical study " disclose the steel slag for climbing steel supply
Main component." improve vanadium slag and produce experiment and the mechanism study of vanadic anhydride leaching rate " of University Of Chongqing is to climbing steel steel slag
Effective purification technique make improvements.Pangang (Group)Panzhihua Iron and Steel Research Institute(PISI) Co., Ltd. is the Technical Research Center for climbing steel,
It has applied for multinomial steel slag vanadium extraction patent, including a kind of method (patent No.: 201611051818), high calcium of Leaching of Vanadium from Vanadium slag
Vanadium slag recovery method (patent No.: 201510282400), the method for the cooling vanadium extraction of Converter Vanadium-bearing Slag (patent No.:
201510848476).Research is also made to steel slag process for extracting vanadium by Chinese Academy Of Sciences Process Engineering Research Institute, with reference to its patent: low
Method (the patent No.: 201510763421.4) of normal temperature and pressure extraction Vanadium in Vanadium Residue and chromium.
These steel slag purifying techniques and vanadine purifying technique of the prior art are mutually indepedent, and purification efficiency is lower.The application
Further improvement is made to this.
Summary of the invention
The invention proposes a kind of methods using steel slag and vanadine mixing vanadium extraction, comprehensively utilize steel slag and vanadine, reduce
Cost improves yield.
The technical scheme of the present invention is realized as follows:
A kind of method of steel slag and the vanadium extraction of vanadine mixture, which comprises the following steps:
1. pretreatment: steel slag is burnt to heat preservation 18 after 1300 to 1400 DEG C to for 24 hours, subsequent rapid cooling to 1000 DEG C or less it is cold
But；
2. being crushed: take steel slag and vanadine, be crushed it is spare, wherein in steel slag contain >=8% V2O5, < 13% SiO2,≤2%
The MnO of CaO and >=5%；
3. milling: steel slag and vanadine are mixed and wear into thin steel slag and thin vanadine, the granularity of thin steel slag and thin vanadine 80 mesh once,
And 100 mesh are to content >=80% of 200 mesh；
4. mixing: score meter by weight takes 30 parts of thin steel slag, thin vanadine mixture and 11 parts of additive to form wet mixing
Raw material；
5. roasting: raw material are put into rotary kiln and are heated, 800 to 850 DEG C of heating temperature, 1 to 2h, generate vanadium bearing slag；
6. leaching: clinker being sent into batch extractor, the feeding after two-stage leaching is de- to be received except miscellaneous filling purifies, and pure leaching is formed
Liquid；
7. precipitation: leachate is passed through vanadium settling tank and reaction kettle, generates ammonium metavanadate and more vanadium after being stood precipitation and heating precipitation
Sour ammonium solid；
8. dry deamination fusing: ammonium metavanadate and ammonium poly-vanadate solid are passed through deamination melting furnace, generate piece of Vanadium.
Preferably, the investment ratio of steel slag and vanadine is 1:5.
Preferably, additive includes 5 parts of cigarette ashes, 2 parts of NaCl, 4 parts of Na2CO3。
Preferably, the liquid-solid ratio of two-stage leaching liquid is 8ml/g.
Preferably, first time leachate is water, and second of leachate is the dilute sulfuric acid that concentration is 2%.
Preferably, leaching pH value 2.8 to 3.0, extraction time 45 to 90 minutes, 50 to 60 DEG C of extraction temperature.
Preferably, drying temperature is 100 to 200 DEG C.
The method for implementing this vanadium extraction of the invention has the advantages that extraction process of the invention can efficiently use
Vanadium iron resources in steel slag are processed as valuable material, are increased economic efficiency, and are reduced energy consumption, are reduced environmental pollution, also
It can promote the development of other relevant industries.Vanadium recovery rate of the present invention reaches 95% or more.The present invention comprehensively utilize vanadine and
Steel slag realizes recycling for vanadium resource, has high economic benefit and social benefit.Contain manganese element in steel slag, vanadium with
Manganese combines in roasting process and forms vanadic acid manganese compound, it is possible to prevente effectively from ring formation phenomenon of the vanadium slag in roasting process, drop
The temperature of low vanadium slag roasting.
Detailed description of the invention
Fig. 1 is the flow chart of the method for steel slag and the vanadium extraction of vanadine mixture of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.
The present invention extracts vanadium piece using the rich vanadium steel slag and vanadine of mixing.Contain TFe, V in rich vanadium steel slag2O5、SiO2、
CaO, MnO etc..SiO2 constitutes the Binder Phase containing vanadic spinel in vanadium slag, and the Binder Phase part is by olivine class Fe2SiO4,
MnSiO4Mineral composition partially exists in the form of tridymite, and the quartz content in vanadium slag is depending on Si in molten iron and blows vanadium condition difference
And have larger fluctuation, there are also a small amount of SiO2With metasilicate such as pyroxene (FeMgCa) OSiO2Or diopside CaMg(SiO3)2Shape
Formula exists.SiO2To the adverse effect of vanadium slag quality.The SiO of low content2Be conducive to the extraction of vanadium.Fe2O3It is often enriched in vanadium slag
At the edge of Spinel, can individually occur, but most of with Fe3O4Form exist.Fe3O4In Fe2O3Due to vanadium slag
Introducing portion FeO can play certain retarding action to the roasting conversion of vanadium slag.Fe in slag2O3It is every to increase by 101%, then FeO in slag
0.45% will be increased, the quantity of slag increases by 1.45%.FeO is in vanadium slag with Fe2+(V3+Cr3+Ti4+Fe3+Al3+) O4And Fe2SiO4Form
It is respectively present in spinelle and silicate phase, is the main composition for constituting vanadium slag, the general > 30% of content.MnO is in vanadium slag
With Mn(V3+Cr3+Ti4+Fe3+) O4And Mn2SiO4Form more uniform be distributed among spinelle and silicate phase.MnO is in slag
In be to be incorporated in by the FeO in replacement slag among above-mentioned object phase.MnO will pass through during the oxidizing roasting of vanadium slag
MnO and Mn2O3Between conversion, to FeO in vanadium slag and V2O3Oxidation play certain catalytic action.
The method of steel slag and the vanadium extraction of vanadine mixture of the invention, comprising the following steps:
1. pretreatment: steel slag is burnt to heat preservation 18 after 1300 to 1400 DEG C to for 24 hours, subsequent rapid cooling to 1000 DEG C or less it is cold
But.
2. being crushed: take steel slag and vanadine, be crushed it is spare, wherein in steel slag contain >=8% V2O5, < 13% SiO2、≤2%
CaO and >=5% MnO.
3. milling: steel slag and vanadine being mixed and wear into thin steel slag and thin vanadine, the granularity of thin steel slag and thin vanadine is in 80 mesh
Once, and content >=80% of 100 mesh to 200 mesh.
4. mixing: score meter by weight takes 30 parts of thin steel slag, thin vanadine mixture and 11 parts of additive to be formed wet
Mixed raw material.Additive includes 5 parts of cigarette ashes, 2 parts of NaCl, 4 parts of Na2CO3。
5. roasting: raw material are put into rotary kiln and are heated, 800 to 850 DEG C of heating temperature, 1 to 2h, generate vanadium bearing slag.
6. leaching: clinker being sent into batch extractor, the feeding after two-stage leaching is de- to be received except miscellaneous filling purifies, and pure leaching is formed
Liquid out.The liquid-solid ratio of two-stage leaching liquid is 8ml/g.First time leachate is water, and second of leachate is dilute sulphur that concentration is 2%
Acid.Leaching pH value 2.8 to 3.0, extraction time 45 to 90 minutes, 50 to 60 DEG C of extraction temperature.
7. precipitation: leachate is passed through vanadium settling tank and reaction kettle, through stand precipitation and heating precipitation after generate ammonium metavanadate and
Ammonium poly-vanadate solid.
8. dry deamination fusing: ammonium metavanadate and ammonium poly-vanadate solid are passed through deamination melting furnace, generate the oxidation of sheet five two
Vanadium.Drying temperature is 100 to 200 DEG C.
Alkalinity additive plays an important role during the oxidizing roasting of vanadium slag, it is the pass for generating soluble vanadium hydrochlorate
Key substance.Alkalinity additive can destroy the former structure containing vanadium mineral, dissociate vanadium from the crystal structure of raw ore object and come, from
And it is oxidized.Alkalinity additive can also accelerate the oxidation of vanadium, improve the roasting conversion rate of vanadium.NaCl chief destructive vanadium mineral
Crystal structure, to vanadium play a part of aoxidize and convert.NaCl can not only improve the oxygenation efficiency of vanadium, and it is anti-to accelerate vanadium oxidation
The phenomenon that progress answered, temperature is higher, and NaCl promotes vanadium oxidation is more obvious.Na in vanadium slag sodium salt system2O amount influences whether vanadium
There are valence state, depressed in identical oxygen, Na2O content is higher, and that there are valence states is higher for vanadium.In the presence of sodium carbonate, maturing temperature
When between 300 ~ 800 DEG C, V can be converted into the sodium salt of water-soluble vanadium, when the temperature is than vanadium titano-magnetite roasting vanadium extraction
Temperature (1050 DEG C) wants much lower.More water-soluble vanadium compounds in order to obtain, the additional amount and maturing temperature of sodium carbonate are
Main determinant, and also by SiO in slag2The influence of content.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of method of steel slag and the vanadium extraction of vanadine mixture, which comprises the following steps:
1. pretreatment: steel slag is burnt to heat preservation 18 after 1300 to 1400 DEG C to for 24 hours, subsequent rapid cooling to 1000 DEG C or less it is cold
But；
2. being crushed: take steel slag and vanadine, be crushed it is spare, wherein in steel slag contain >=8% V2O5, < 13% SiO2,≤2%
The MnO of CaO and >=5%；
3. milling: steel slag and vanadine are mixed and wear into thin steel slag and thin vanadine, the granularity of thin steel slag and thin vanadine 80 mesh once,
And 100 mesh are to content >=80% of 200 mesh；
4. mixing: score meter by weight takes 30 parts of thin steel slag, thin vanadine mixture and 11 parts of additive to form wet mixing
Raw material；
5. roasting: raw material are put into rotary kiln and are heated, 800 to 850 DEG C of heating temperature, 1 to 2h, generate vanadium bearing slag；
6. leaching: clinker being sent into batch extractor, the feeding after two-stage leaching is de- to be received except miscellaneous filling purifies, and pure leaching is formed
Liquid；
7. precipitation: leachate is passed through vanadium settling tank and reaction kettle, generates ammonium metavanadate and more vanadium after being stood precipitation and heating precipitation
Sour ammonium solid；
8. dry deamination fusing: ammonium metavanadate and ammonium poly-vanadate solid are passed through deamination melting furnace, generate piece of Vanadium.
2. the method for vanadium extraction according to claim 1, which is characterized in that the investment ratio of steel slag and vanadine is 1:5.
3. the method for vanadium extraction according to claim 1 or 2, which is characterized in that additive includes 5 parts of cigarette ashes, 2 parts
NaCl, 4 parts of Na2CO3。
4. the method for vanadium extraction according to claim 1 or 2, which is characterized in that the liquid-solid ratio of two-stage leaching liquid is 8ml/g.
5. the method for vanadium extraction according to claim 4, which is characterized in that first time leachate is water, second of leachate
The dilute sulfuric acid for being 2% for concentration.
6. the method for vanadium extraction according to claim 4, which is characterized in that leach pH value 2.8 to 3.0, extraction time 45 to
90 minutes, 50 to 60 DEG C of extraction temperature.
7. the method for vanadium extraction according to claim 1 or 2, which is characterized in that drying temperature is 100 to 200 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111186859A (en) * | 2019-12-20 | 2020-05-22 | 大连博融新材料有限公司 | Superfine V2O5Powder, method for the production thereof and use thereof |
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| CN107236871A (en) * | 2017-06-22 | 2017-10-10 | 河钢股份有限公司承德分公司 | A kind of method for mixing vanadium slag and v-bearing steel slag pressurization vanadium extraction |
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2018
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102251119A (en) * | 2011-07-04 | 2011-11-23 | 中国科学院过程工程研究所 | Method for recycling vanadium extraction tailings |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111186859A (en) * | 2019-12-20 | 2020-05-22 | 大连博融新材料有限公司 | Superfine V2O5Powder, method for the production thereof and use thereof |
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Application publication date: 20190409 |